HRID742338

反应详情

EQUATION

反应方程式

HRID 742338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

4-t-Butylaniline (14.9 g, 100 mmol) was suspended in aqueous hydrochloric acid (50 ml, 6M) at 5° C. Sodium nitrite (7.6 g, 110 mmol in 10 ml water) was added at such a rate that the temperature was kept between 5°-7° C. Following the addition the resulting solution was stirred for 15 min. and sodium tetrafluoroborate (15.4 g, 140 mmol in 30 ml water) was added at 5-8° C. The mixture was stirred for 15 min. 4-t-Butylbenzenediazonium tetrafluoroborate was filtered off, dried with suction and washed with diethyl ether to yield 20.96 g. This diazonium salt was decomposed by heating to 140° C. on an oil-bath. The product was distilled off at reduced pressure. Yield 11.15 g colorless oil.

WORKUP

后处理

  1. customwas kept between 5°-7° C
  2. additionthe addition the resulting solution
  3. stirringThe mixture was stirred for 15 min
  4. filtration4-t-Butylbenzenediazonium tetrafluoroborate was filtered off
  5. customdried with suction
  6. washwashed with diethyl ether
  7. customto yield 20.96 g
  8. distillationThe product was distilled off at reduced pressure